Manufacture of metallic amids, cyanamids, and cyanids.



E. A. ASHCROFT.

MANUFACTURE 0rr METALLIC AIVIIDS, CYANAIVIIDS, AND CYANIDS.

APPLICATION FILED APR. I4. ISIO.

,L63,4:9. Patented Dec. T, 1915.

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EDGAR ARTHUR ASHCROFT, 0F LQNDON, GLANID.

Specification of lLetters Patent.

patenten nec.. 'a i915.

Application filed April 14:, 1910. Serial No. 555,530.

Be it known that I, EDGAR ARTHUR ASH- onorr, a subject of the King' of Great Britain and Ireland, of 99 Buckingham Palace road, in the county of London, England, have invented new and useful Improvements in the Manufacture of Metallic Amids, Cyanamids, and Cyanids, of which the following is aspeCiiCatiOn.

My invention relates to the direct production, by electrolysis, of amide, cyanamids, and cyanids, of the alkali metals, Such for example as sodium, or potassium, from raw materials, (such as the chlorids, or hydrates, of alkali metals) and nitrogenous matter or both nitrogenous matter and carbon, or carbonaceous gas, accordingI to whether amids, cyanamids, or cyanide, are to be produced.

It has long been known thatif nitrogenous mattei', such as ammonia gas, be brought into contact with metallic sodium, at a temperature above the melting point of sodium amid (120 centigrade), and below its decomposition point (about 440 centigrade), fused sodium amid will readily be produced, the reaction being and that' this amid, if. brought into contact with carbon, or carbonaceous gas, such as acetylene, or coal `gas, at a temperature above 350 centigrade and below 600 centigrade, will yield disodium cyanamid, the reaction being It is also known that sodium amid in contact with""sodium cyanid at a temperature just above 400 centigrade will react and yield disodium cyanamid according to the reaction v and that disodium cyanamid will react with' carbon at a temperature of about 800 centigrade and form cy'anid, the reaction being or tin, or an allow tion of sodium amid by injecting ammonia in conseinto the molten allo-y, and also to produce Y the said alloy continuously by'electrolysis,"

have discovered that either amids, cy-

anamids, or cyanide,

duced according` "to a new process based upon the process described inthe specification of United States Patent 801199 dated the 10th October 1905 granted ,to me. A v

In carrying the process according to my present invention into effect (taking the production of sodium derivatives as an example), I employ a double cell apparatus and an intermediate electrode of a molten vmetal, such, for example, as lead, mercury, of any of these, (and I may add any other suitable metal), with which is alloyed the sodium produced in the first cell, and then this intermediate electrode is conveyed to the second cell of the alkali metals, can be economically and conveniently prowhere it is subjected to anode reactions, as

described in the specification of my laforesaid Patent No. 801199, but, in carrying out my present invention, may use, in the first cell, other raw materials than the chlorid of the desired metal, such, for instance, as thehydrate of sodium (caustic soda), or the sulid of sodium,either alone, or in any suitable admixture with luxing material, such as sodium, or potassium, chlorid, iodid, or the like, and in the second celll, substitute for the electrolytes recommended for the production of alkali metals in accordance with my aforesaid Patent No. 801,199, an electrolyte consisting of fused amid, cyanamid, or cyanid, or the 11ke,of the metal'under consideration, for instance, sodium amid alone, ory in various admugtures, according" to the product which 1t 1s desired to obtain. ployed for the 'intermediate electrode, I may use a solution of the raw materia-l, such as chlorid of sodium, or the like, as the electrolyte in the first cell.. If sodium amid` for example, be the product which is to be obtained by the process of my present invention, anhydrous ammonia in the lform ot' gas is conducted into the second cell through any convenient pipe, Vor through a hollow cathode, and this ammonia gas, by coming When mercury is em- 40 i cedure is the same asin making the cyanin contact with the nascent sodium pro-- duced, forms more NaNHzil-H (the .hydrogen escaping) and thus continuously aug ments the electrolyte' which is periodically tapped olf for use for any desired purpose.

In ltheoperation it is desirable, in order to secure maximum efficiency and avoid loss of ammonia, to keep the temperature of the g second cell as low as possible consistent with .the free mdvement of the anode alloy, av

temperature of, say, between 250 and 350:7 centigrade being suitable, the higher temperatures "being necessary when a fused,

electrolyte is used in the first cell and an intermediate electrode of lead alloy, the Alower temperatures being preferable when a f solution of the raw .materialsis used in the terials, must be used in the first cell, and

lso

mercury is not suitable for the intermediate electrode. At the start, the electrolyte may be introduced into the cell as cyanamid, or s the/cyanamid may be formed in the cell by means of ammonia. and carbon. The tem'- perature employed in the second cell in this case will be somewhat higher (say 500o centigrade), especially toward the end of the reaction and previous to drawing a charge, so that the produced cyanamid remains fused and mobile and can be tapped off 4pelriodically.

` When cyanid is to begproduced, the promaands, except that the temperature is raised to or about 800 centigrade, preferably to- Ward the end of the reaction and before drawing off a charge, and that more carbon is added. Instarting the process, the electrolyte may be introduced into the cell as cyanid, or the cyanid may be formed in the celll by causing carbon and' ammonia to react economical advantages over the hithertol with the nascent sodium. u It will be evident that the process accordlng to my present invention presents great -known 'methods of producing amids, cyanamids, and cyamds, as 1t constitutes a contin nous process for the v'manufacture of the "said products direct from the raw materials (such, for example, as sodium chlorid, or caustic soda)y with ammonia, or ammonia and carbon.

Considering the present industry as a Whole whereby sodium metal, for example, is first produced electrolytically and after- Vward employed according to the Aknown -methods for making the desired products,

myr present invention avoids all the labor and other costs of collecting and packing the metal and re-treating it in separate apparatus heated externally.

Even when, in carrying out my present I invention, caustic soda is employed as the being eliminated largely as steam and not decomposed by the current), and partly because of the avoidance, as aforesaid, of much labor and other items of cost in separate sodium production, and collection, packing, and the like. i

In the accompanying diagrammatic illustration, the first cell may contain as electrolyte sodium chlorid or sodium hydroXid, the cathode being alkali metal lead alloy. The alkali metal lead alloy which may be sodium-lead passes during the operation of the process into the second cell where it becomes the anode, the electrolyte in the second cell being the desired product.

As will be seen from the illustration, chlorin, or watery vapor (steam) plus oxygen escapes from the first cell while hy# drogen escapes from the second cell, ammonia being introduced into the second cell to obtain the required reaction and the depleted sodium-lead alloy being continuously returned to th'e first cell.

Vhen a fused halogen salt is the raw material used in the first cell, anodes of graphite or carbon, are most suitable forthis cell, chlorin, escaping. When caustic soda is the raw material employed, anodes of nickel are most suitable. When I use solutions of the raw materials, such as a soluf tion of sodium chlorid, the anodes may be of graphite, or of platinum, which may, for

instance,l be inthe form( of`gauze. The.

cathode in the second cell may be of copper, or nickel, or other suitable material, and the containing vessel may be made of coppe-n nickel, iron, or the like.

Although I have described the invention as being carried out from the raw materials, it will be understood that, if desired, the alloy constituting the aforesaid intermediate electrodeI mayV be taken from any other source and used as the anode in carrying out the process of the production of amid, cyanamid, or cyanid, as described with regaid to the action in the aforesaid second ce It will be evident that, in place of using ammonia I may employ other suitable nitrogenous matter.

It is to be understood that, in followsodium, potassium,

pounds of alkali What I claim i in mentioning the commetals especially those of and ymixtures thereof.

13. l. The process of producing nitrogencontaining comp alkali-earth ounds of the alkali and metals which consists in subjecting a fused bath consisting substantially entirely of p roduct to electr the desired nitrogen-.containing v olysis over an anode consisting of an alloy of'said metal and in the presence of an agent reacting with the nascent metal at the cathode to form the desired nitrogen-containing product.

2. A cyclic process for producing nitrogen-containing compounds alkali-earth metals,

jecting suitable r in a irst cell ove of 4the alkali and which consists in suhaW material to electrolysis r a metal cathode adapted to become alloyedwith the said metal yielded by the raw material, electrolyzing said alloy as anode in a second cell having as its electrolyte substantially solely` the desired nitrogen-containing product and introducing into said second cell a nitrogencontaining radical to react with the `nascent metal produced at desired nitrogen-containing compound, and

vreturning the depleted alloy to the first cell EDGAR Ain-HUB Astronom. lWitnesses EDWARD GEORGE Davies, I-I. I). JAMESON.

Copies of this patent may be obtained fer ve cents each, by addressing the "Commissioner of Patents,

' Washington. D. G. 

